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低电子能量下电子透明样品中的电子束展宽

Electron beam broadening in electron-transparent samples at low electron energies.

作者信息

Hugenschmidt M, Müller E, Gerthsen D

机构信息

Laboratory for Electron Microscopy (LEM), Karlsruhe Institute of Technology (KIT), Engesserstr. 7, 76131, Karlsruhe, Baden-Württemberg, Germany.

出版信息

J Microsc. 2019 Jun;274(3):150-157. doi: 10.1111/jmi.12793. Epub 2019 May 2.

Abstract

Scanning transmission electron microscopy (STEM) at low primary electron energies has received increasing attention in recent years because knock-on damage can be avoided and high contrast for weakly scattering materials is obtained. However, the broadening of the electron beam in the sample is pronounced at low electron energies, which degrades resolution and limits the maximum specimen thickness. In this work, we have studied electron beam broadening in materials with atomic numbers Z between 10 and 32 (MgO, Si, SrTiO , Ge) and thicknesses up to 900 nm. Beam broadening is directly measured using a multisegmented STEM detector installed in a scanning electron microscope at electron energies between 15 and 30 keV. For experimental reasons, the electron beam diameter is defined to contain only 68% of the total intensity instead of the commonly used 90% of the total beam intensity. The measured beam diameters can be well described with calculated ones based on a recently published model by Gauvin and Rudinsky. Using the concept of anomalous diffusion the Hurst exponent H is introduced that varies between 0.5 and 1 for different scattering regimes depending on t/Λ with the specimen thickness t and the elastic mean free path length Λ . The calculations also depend on the fraction of the beam intensity that defines the electron beam diameter. A Hurst exponent H of 1 is characteristic for the ballistic scattering regime with t/Λ → 0 and can be excluded for the experimental conditions of our study with 6 ≦ t/Λ ≦ 30. We deduced H = 0.75 from measured beam diameters which is larger than H = 0.5 that is expected under diffusion conditions. The deviation towards larger H values can be rationalised by our definition of electron diameter that contains only 68% of the total beam intensity and requires therefore larger sample thicknesses before the diffusion regime is reached. Our results clearly deviate from previous analytical approaches to describe beam broadening (Goldstein et al., Reed, Williams et al., Kohl and Reimer). Measured beam diameters are compared with simulated ones, which are obtained by solving the electron transport equation. This approach is advantageous compared to the commonly used Monte Carlo simulations because it is an exact solution of the electron transport equation and requires less computer time. Simulated beam diameter agree well with the experimental data and yield H = 0.80. LAY DESCRIPTION: In scanning transmission electron microscopy (STEM), a focused electron beam is scanned over an electron-transparent sample and an image is formed by detecting the intensity of the transmitted electrons by a STEM detector. STEM resolution is ultimately limited by the electron beam diameter and can be better than 0.1 nm for the best microscopes. However, the electron-beam diameter increases with increasing specimen thickness because electrons are scattered by the interaction of the specimen material and electrons. Electron scattering leads to a change of the electron propagation direction and reduces focusing of the electron beam. The associated electron-beam broadening degrades the lateral resolution of STEM and generally limits the maximum specimen thickness that can be imaged with good resolution. STEM is up to now mainly performed at high electron energies of 80 keV and above. Lower electron energies are beneficial for the study of weakly scattering and radiation-sensitive materials but electron beam broadening becomes more pronounced with decreasing electron energies. Knowledge of beam broadening is therefore particularly important for the interpretation of STEM images that are taken with low-energy electrons. In this work we have studied electron-beam broadening in different materials with thicknesses up to 900 nm at low electron energies between 15  and 30 keV. Beam broadening is directly measured with a newly developed technique. We compare measured beam diameters with different models on beam broadening from literature and find that only a recently published model is well suited to describe the experimental results under our experimental conditions. In addition, beam broadening is simulated by modelling electron propagation in the specimen. The simulation results agree well with the measured beam diameters.

摘要

近年来,低初级电子能量的扫描透射电子显微镜(STEM)受到了越来越多的关注,因为可以避免碰撞损伤,并且对于弱散射材料可获得高对比度。然而,在低电子能量下,样品中电子束的展宽很明显,这会降低分辨率并限制最大样品厚度。在这项工作中,我们研究了原子序数Z在10到32之间的材料(MgO、Si、SrTiO₃、Ge)中电子束的展宽情况,样品厚度可达900 nm。使用安装在扫描电子显微镜中的多段STEM探测器,在15至30 keV的电子能量下直接测量电子束展宽。出于实验原因,电子束直径被定义为仅包含总强度的68%,而不是常用的总束强度的90%。基于Gauvin和Rudinsky最近发表的模型计算得到的束直径能够很好地描述测量值。利用反常扩散的概念引入了赫斯特指数H,根据样品厚度t和弹性平均自由程长度Λ,在不同散射区域中,H在0.5到1之间变化。计算还取决于定义电子束直径的束强度分数。赫斯特指数H为1是t/Λ→0时弹道散射区域的特征,在我们6≦t/Λ≦30的实验条件下可以排除这种情况。我们从测量的束直径推导出H = 0.75,这大于扩散条件下预期的H = 0.5。向更大H值的偏差可以通过我们对仅包含总束强度68%的电子直径的定义来解释,因此在达到扩散区域之前需要更大的样品厚度。我们的结果明显偏离了以往描述束展宽的分析方法(Goldstein等人[1977]、Reed[1985]、Williams等人[1989]、Kohl和Reimer[1998])。将测量的束直径与通过求解电子输运方程得到的模拟值进行比较。与常用的蒙特卡罗模拟相比,这种方法具有优势,因为它是电子输运方程的精确解,并且所需的计算机时间更少。模拟的束直径与实验数据吻合良好,得到H = 0.80。

层面描述

在扫描透射电子显微镜(STEM)中,聚焦电子束在电子透明样品上扫描,并通过STEM探测器检测透射电子的强度来形成图像。STEM分辨率最终受电子束直径限制,对于最好的显微镜,分辨率可以优于0.1 nm。然而,电子束直径会随着样品厚度的增加而增大,因为电子会因样品材料与电子的相互作用而发生散射。电子散射会导致电子传播方向改变,降低电子束的聚焦程度。相关的电子束展宽会降低STEM的横向分辨率,通常会限制能够以高分辨率成像的最大样品厚度。到目前为止,STEM主要在80 keV及以上的高电子能量下进行。较低的电子能量有利于研究弱散射和对辐射敏感的材料,但电子束展宽会随着电子能量的降低而变得更加明显。因此,了解束展宽对于解释用低能电子拍摄的STEM图像尤为重要。在这项工作中,我们研究了在15至30 keV的低电子能量下,不同材料中厚度达900 nm的电子束展宽情况。使用一种新开发的技术直接测量束展宽。我们将测量的束直径与文献中不同的束展宽模型进行比较,发现只有最近发表的模型非常适合描述我们实验条件下的实验结果。此外,通过对样品中电子传播进行建模来模拟束展宽。模拟结果与测量的束直径吻合良好。

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